The semiconducting compound has been recognized as a thermoelectric material with excel-lent oxidation resistance and stable characteristics at elevated temperature. In the present work, we applied mechanical alloying(MA) technique to produce compound using a mixture of elemental iron and silicon powders. The mechanical alloying was carried out using a Fritsch P-5 planetary mill under Ar gas atmosphere. The MA powders were characterized by the X-ray diffraction with Cu-K radiation, thermal analysis and scanning electron microscopy. The single phase has been obtained by mechanical alloying of mixture powders for 120 hrs or for 70 hrs coupled with the subsequent heat treatment up to . The grain size of powders analyzed by Hall plot method was 44nm.